CN114152489B - Platinum-palladium-gold gray blowing method in black rock by taking tellurium-silver as protective agent - Google Patents
Platinum-palladium-gold gray blowing method in black rock by taking tellurium-silver as protective agent Download PDFInfo
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- 239000010931 gold Substances 0.000 title claims abstract description 64
- 229910052737 gold Inorganic materials 0.000 title claims abstract description 63
- 238000007664 blowing Methods 0.000 title claims abstract description 57
- 239000011435 rock Substances 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 27
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 26
- 239000004332 silver Substances 0.000 title claims abstract description 26
- 239000003223 protective agent Substances 0.000 title claims abstract description 11
- 238000012360 testing method Methods 0.000 claims abstract description 54
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 36
- AJZRPMVVFWWBIW-UHFFFAOYSA-N [Au].[Bi] Chemical compound [Au].[Bi] AJZRPMVVFWWBIW-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052797 bismuth Inorganic materials 0.000 claims description 31
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 31
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 24
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 20
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 16
- 229910021538 borax Inorganic materials 0.000 claims description 14
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 14
- 239000004328 sodium tetraborate Substances 0.000 claims description 14
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 12
- 235000010333 potassium nitrate Nutrition 0.000 claims description 12
- 239000004323 potassium nitrate Substances 0.000 claims description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 11
- 229910000416 bismuth oxide Inorganic materials 0.000 claims description 11
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 claims description 11
- 239000004615 ingredient Substances 0.000 claims description 11
- 239000004927 clay Substances 0.000 claims description 9
- 239000000395 magnesium oxide Substances 0.000 claims description 9
- 235000013339 cereals Nutrition 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000002844 melting Methods 0.000 claims description 7
- 230000008018 melting Effects 0.000 claims description 7
- 101710134784 Agnoprotein Proteins 0.000 claims description 6
- 229910004273 TeO3 Inorganic materials 0.000 claims description 6
- 235000013312 flour Nutrition 0.000 claims description 6
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 6
- 241000209140 Triticum Species 0.000 claims description 5
- 235000021307 Triticum Nutrition 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical group [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 5
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 5
- 239000000377 silicon dioxide Substances 0.000 claims description 5
- 235000012239 silicon dioxide Nutrition 0.000 claims description 5
- 229910052573 porcelain Inorganic materials 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 235000017550 sodium carbonate Nutrition 0.000 claims description 2
- 229910052697 platinum Inorganic materials 0.000 abstract description 19
- 238000005259 measurement Methods 0.000 abstract description 12
- 238000004458 analytical method Methods 0.000 abstract description 9
- 238000001514 detection method Methods 0.000 abstract description 6
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 abstract description 6
- 239000002245 particle Substances 0.000 abstract description 5
- 239000002253 acid Substances 0.000 abstract description 4
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 4
- 229910001316 Ag alloy Inorganic materials 0.000 abstract description 3
- 230000006378 damage Effects 0.000 abstract description 3
- 239000007800 oxidant agent Substances 0.000 abstract description 3
- 208000027418 Wounds and injury Diseases 0.000 abstract description 2
- 238000005485 electric heating Methods 0.000 abstract description 2
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 208000014674 injury Diseases 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000000155 melt Substances 0.000 abstract description 2
- 239000010970 precious metal Substances 0.000 abstract description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 24
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 19
- 229910000510 noble metal Inorganic materials 0.000 description 19
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 13
- 229910052799 carbon Inorganic materials 0.000 description 13
- 239000000126 substance Substances 0.000 description 11
- 229910052759 nickel Inorganic materials 0.000 description 10
- 238000002474 experimental method Methods 0.000 description 9
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 8
- 230000000694 effects Effects 0.000 description 8
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 8
- 239000002893 slag Substances 0.000 description 8
- 238000011084 recovery Methods 0.000 description 7
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 6
- 239000011246 composite particle Substances 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 4
- 229910052763 palladium Inorganic materials 0.000 description 4
- 229910001961 silver nitrate Inorganic materials 0.000 description 4
- 229910052717 sulfur Inorganic materials 0.000 description 4
- 239000011593 sulfur Substances 0.000 description 4
- 238000010998 test method Methods 0.000 description 4
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 description 3
- 239000011324 bead Substances 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- BFPJYWDBBLZXOM-UHFFFAOYSA-L potassium tellurite Chemical compound [K+].[K+].[O-][Te]([O-])=O BFPJYWDBBLZXOM-UHFFFAOYSA-L 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 231100000053 low toxicity Toxicity 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- YFLLTMUVNFGTIW-UHFFFAOYSA-N nickel;sulfanylidenecopper Chemical compound [Ni].[Cu]=S YFLLTMUVNFGTIW-UHFFFAOYSA-N 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 238000010561 standard procedure Methods 0.000 description 2
- 239000012086 standard solution Substances 0.000 description 2
- 239000011550 stock solution Substances 0.000 description 2
- -1 sulfonium nickel gold Chemical compound 0.000 description 2
- 229910052714 tellurium Inorganic materials 0.000 description 2
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000012224 working solution Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229910003296 Ni-Mo Inorganic materials 0.000 description 1
- RWDMAZGBOZOYKZ-UHFFFAOYSA-N [Fe+2].[N+](=O)([O-])[O-].[K+].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-] Chemical compound [Fe+2].[N+](=O)([O-])[O-].[K+].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-] RWDMAZGBOZOYKZ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000011088 calibration curve Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- JUWSSMXCCAMYGX-UHFFFAOYSA-N gold platinum Chemical compound [Pt].[Au] JUWSSMXCCAMYGX-UHFFFAOYSA-N 0.000 description 1
- JVPLOXQKFGYFMN-UHFFFAOYSA-N gold tin Chemical compound [Sn].[Au] JVPLOXQKFGYFMN-UHFFFAOYSA-N 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 1
- 229910001867 inorganic solvent Inorganic materials 0.000 description 1
- 239000003049 inorganic solvent Substances 0.000 description 1
- 238000012417 linear regression Methods 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- DDTIGTPWGISMKL-UHFFFAOYSA-N molybdenum nickel Chemical compound [Ni].[Mo] DDTIGTPWGISMKL-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B11/00—Obtaining noble metals
- C22B11/02—Obtaining noble metals by dry processes
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
- G01N27/626—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using heat to ionise a gas
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The invention discloses a platinum-palladium-gold ash blowing method in black rock with tellurium-silver as a protective agent, which aims at improving a bismuth gold test formula according to the characteristics of the black rock, adding a proper oxidizing agent KNO 3 to improve a reducing medium of a melt, using Ag-Te as an ash blowing protective agent, adopting secondary ash blowing-open dissolved tellurium-silver alloy particle-ICP-AES to measure Pt, pd and Au in a black rock sample, and solving the problems of poor reproducibility and low accuracy of a measurement result caused by the fact that the conventional gold test formula is not buckled or not beaded. The method is strong in operability, precious metal tellurium-silver particles can be digested on the electric heating plate by using a small amount of acid, so that the analysis flow is greatly shortened, reagents and energy are saved, environmental pollution and injury to operators are reduced, the production cost is effectively reduced, the analysis and detection efficiency is improved, and the method can be applied to determination of Pt, pd and Au in a large amount of black rock samples.
Description
Technical Field
The invention belongs to the technical field of precious metal recovery, and particularly relates to a platinum-palladium-gold gray blowing method in black rock by taking tellurium-silver as a protective agent.
Background
Noble metals are widely used in the fields of electronics, communication, aerospace, chemical industry, medical industry and modern high and new technology industry due to excellent physical and chemical properties and unique catalytic activity. In terms of economic value, its unique monetary attributes are often used as national financial reserves. In the field of ornaments, demands are increasing year by year due to attractive appearance and warranty. With the progress of exploration means, geologists have recently found platinum group elements in black rock, and this result is expected to alleviate the current situation of shortage of platinum group resources. However, the black rock contains a large amount of carbon, organic carbon and sulfide, and the complex components and the reduction characteristics of the black rock increase the difficulty in analyzing noble metals and other elements in the black rock.
Currently, methods for noble metal analysis mainly include a wet method and a fire gold test method. The wet method mainly adopts aqua regia, HCl-H 2O2、HCl-H2O2-KClO3 and other inorganic solvents to open or close under high pressure to digest the sample. However, the black rock sample contains a large amount of free carbon and organic carbon, and reports indicate that the volatilization loss of noble metal elements can be caused by the carbon removal by burning. And by adopting a direct digestion mode, a large amount of carbon cannot be digested, and the noble metal element has a strong adsorption effect, so that the result is seriously lower. The fire gold test method is to collect noble metal by high temperature smelting method, and has the advantages of good sampling representativeness, wide applicability, good enrichment effect, etc., and common collecting modes include sulfonium nickel gold test, lead gold test, tin gold test, bismuth gold test, etc. Nickel matte gold test is a gold test method which is gradually mature in the 90 th century of the 20 th century and can simultaneously collect Pt, pd, rh, ir, os, ru six platinum group elements, and a national standard method (GB/T17418.7-2010) is formed. However, the gold test of nickel matte is not ideal in trapping effect on Au, and cannot quantitatively trap platinum group elements in black rock due to the influence of carbon and organic matters. Tin test developed in Gong th and so on can accurately measure eight noble metal elements in black rock, but the flow of tin test is long, and the cost is high (Gongling, li Zhiwei, wang Minjie, and so on). Lead gold test is a classical fire gold test method, forms a plurality of standard methods aiming at different minerals, is also an internationally accepted general method, can simultaneously capture gold, silver, platinum and palladium, and can rapidly blow ash in a cupel, and the method is simple and convenient and has high efficiency. However, due to the volatilization of a large amount of lead, serious pollution and damage are caused to the environment and human body, and the existence of a large amount of carbon is easy to crust during ash blowing, so that the beading effect is poor. Zhang Danlin, li Keji and the like adopt bismuth test to trap noble metals, and the bismuth is easy to blow ash and has low toxicity, so that the requirements of energy-saving and environment-friendly analytical chemistry are met (Zhang Danlin, tu Huimin. Research on noble metals in bismuth test enriched ores [ J ] mineral and geology, 1981, (2): 90-102; li Keji, zhao Chaohui, fan Jianxiong. Trace gold platinum palladium [ J ] metallurgical analysis in poor platinum ores is determined by bismuth test-inductively coupled plasma mass spectrometry, 2013, 33 (8): 19-23.). However, the buckling stability and the ash blowing condition are still not perfect, so that the black rock sample cannot be popularized, and particularly gold and silver beads cannot be formed basically when ash blowing is performed on the black rock sample.
In view of this, the present invention has been made.
Disclosure of Invention
Aiming at the problems, the invention provides a platinum-palladium-gold gray blowing method in black rock, which takes tellurium-silver as a protective agent, improves a bismuth gold test formula according to the characteristics of the black rock, adds a proper oxidant KNO 3 to improve a reducing medium of a melt, uses Ag-Te as a gray blowing protective agent, adopts secondary gray blowing-open dissolving tellurium-silver alloy particles-ICP-AES to measure Pt, pd and Au in black rock samples, has the recovery rate of more than 97 percent, has low detection limit and high analysis efficiency, and can be applied to the measurement of Pt, pd and Au in a large number of black rock samples.
In order to solve the technical problems, the invention adopts the following technical scheme:
a platinum-palladium-gold gray blowing method in black rock with tellurium-silver as a protective agent comprises the following steps:
(1) Enrichment of bismuth gold test: adding a gold test ingredient into 10.0g of black shale sample, dropwise adding 0.5ml of 60g/L AgNO 3 solution and 0.5ml of 76g/L K 2TeO3 solution, fully and uniformly mixing, pouring into a clay crucible, uniformly adding a layer of SiC and light MgO mixed covering agent, placing the clay crucible into a gold test furnace at 800 ℃, heating for 20min, continuously heating to 1100 ℃ for melting for 30min, taking out the crucible while the crucible is hot, pouring the molten mass into an iron mold, smashing a glass body after cooling, and taking out a bismuth buckle;
(2) Primary ash blowing: preheating a magnesia cupel in a high-temperature furnace at 900 ℃ for 1h, taking out, immediately placing a bismuth button in the cupel, putting the cupel in the high-temperature furnace again, adjusting the furnace temperature to 860 ℃, closing the furnace door for 1-2 min, opening the furnace door for 2-3 cm, leading air into a furnace chamber, and carrying out primary ash blowing;
(3) Secondary ash blowing: when the primary ash blowing is about to end, placing a ceramic crucible containing 2-3 g of borax into a high-temperature furnace for melting, rapidly pouring bismuth buckles into the ceramic crucible containing molten borax when the bismuth buckle ash is blown to the diameter of 5mm, continuing secondary ash blowing, taking out the crucible when the grain mixing diameter is 1-2 mm, naturally cooling, crushing, and taking out tellurium-silver grains.
Further, the gold test ingredients in the step (1) consist of borax, sodium carbonate, silicon dioxide, bismuth oxide, wheat flour, potassium nitrate, iron powder and a covering agent, and 15g of borax, 50g of sodium carbonate, 10g of silicon dioxide, 40g of bismuth oxide, 2g of wheat flour, 15g of potassium nitrate, 8g of iron powder and 5g of covering agent are needed based on 10.0g of black shale sample.
The invention has the beneficial effects that: the bismuth oxide with low toxicity is used as a trapping agent, the property of black rock sample slag is improved through adjusting a gold test formula, particularly AgNO 3 solution and K 2TeO3 solution are added, and the bismuth oxide is combined with noble metal at high temperature to form smooth and round tellurium-silver aggregate, so that the problems of poor repeatability and low accuracy of a measurement result caused by the fact that a conventional gold test formula is not buckled and is not blown into beads are solved. The method is strong in operability, the noble metal tellurium-silver composite particles can be digested on the electric heating plate by using a small amount of acid, the analysis flow is greatly shortened, reagents and energy sources are saved, the environmental pollution and the injury to operators are reduced, the production cost is effectively reduced, the analysis and detection efficiency is improved, and the method is suitable for measuring trace amounts, trace amounts of Pt, pd and Au in a large batch of black rock samples.
Drawings
Fig. 1 shows the loose silver flakes after one ash blow.
Fig. 2 shows the tellurium-silver composite particles after secondary ash blowing.
FIG. 3 shows the effect of potassium nitrate usage on primary ash blowing.
Fig. 4 shows the secondary ash blowing of bismuth buckles with silver nitrate.
Fig. 5 shows the secondary ash blowing of bismuth buckles with the addition of silver nitrate and potassium tellurite.
Detailed Description
The present invention will be further described with reference to specific examples, but the scope of the present invention is not limited thereto.
Example 1
The instruments and reagents used in this example are as follows:
the operating conditions of the iCAP6300 Radial inductively coupled plasma atomic emission spectrometer (ICP-AES, thermo company, usa) are shown in table 1.
TABLE 1 ICP AES working conditions
A gold test furnace (Luoyang torch Star kiln furnace Co., ltd.) GWL-1400 ℃;
a gold test crucible (clay);
magnesia cupel.
The main reagents used in this example were as follows:
Silver nitrate (AgNO 3): 60.0g/L; potassium tellurite (K 2TeO3): 76.0g/L; covering agent: silicon carbide + light magnesia; hydrochloric acid, nitric acid, sodium carbonate and silicon dioxide are analytically pure; borax and bismuth oxide are chemically pure; the water for the experiment is deionized water.
Au, pt, pd standard solutions: standard stock solutions of 1.000mg/mL were formulated with metals Au, pt, pd of spectroscopic purity or greater than 99.99% (mass fraction). Standard stock solutions containing Au, pt and Pd are diluted step by step to prepare mixed standard working solution with rho (Au, pt and Pd) =10.0 mug/mL, and the medium is aqua regia with the concentration of 5% (V/V).
The platinum-palladium-gold gray blowing method in the black rock taking tellurium and silver as the protective agent comprises the following steps:
(1) Bismuth gold test enrichment
Accurately weighing 10.0g of black shale sample, adding a gold test ingredient according to Table 2, dropwise adding 0.5mL of 60g/L AgNO 3 solution and 0.5mL of 76g/L K 2TeO3 solution, fully and uniformly mixing, pouring into a clay crucible, and uniformly adding a layer of SiC and light MgO mixed covering agent. And (3) placing the clay crucible in a gold test furnace at 800 ℃ for heating for 20min, continuously heating to 1100 ℃ for melting for 30min, taking out the crucible while the clay crucible is hot, pouring the molten mass into an iron mold, cooling, smashing the glass body, and taking out the bismuth buckle.
TABLE 2 flux formulation for gold test
| Sample preparation | Sampling amount | Borax | Sodium carbonate | Silica dioxide | Bismuth oxide | Wheat flour | Potassium nitrate | Iron powder | Covering agent |
| Black shale | 10g | 15g | 50g | 10g | 40g | 2g | 15g | 8g | 5g |
(2) Two times of ash blowing
The magnesia cupel is placed in a high-temperature furnace at 900 ℃ for preheating for 1h, taken out, immediately placed in the cupel, put in the high-temperature furnace again, the furnace temperature is regulated to 860 ℃, after the furnace door is closed for 1-2 min, the furnace door is opened for 2-3 cm, so that air is introduced into a furnace chamber, and ash blowing is carried out once. When the primary ash blowing is about to end, placing a ceramic crucible containing 2-3 g of borax into a high-temperature furnace for melting, rapidly pouring bismuth buckles into the ceramic crucible containing molten borax when the bismuth buckle ash is blown to the diameter of about 5mm, continuing secondary ash blowing, taking out the crucible when the grain mixing diameter is 1-2 mm, naturally cooling, crushing, and taking out tellurium-silver grains.
Dissolution and measurement of the syncytia: putting tellurium-silver alloy particles into a 50mL small beaker, adding 5mL of 1+3 nitric acid, heating and dissolving on an electric plate at 150 ℃, adding 5mL of concentrated HCl until the alloy particles do not bubble, continuously heating and dissolving until the alloy particles are completely decomposed, taking down and cooling, fixing the volume into a 10mL colorimetric tube by using 10% hydrochloric acid, and shaking uniformly. ICP-AES measures the content of Pt, pd and Au.
1. Selection of test ingredients
The fire test and the deduction have close relation with the sample composition and the selection and the proportion of the test ingredients. Because the black rock sample contains higher carbon, organic carbon, a large amount of metal sulfides and other components, the slag with better fluidity and a smooth and complete gold testing buckle cannot be obtained by adopting a gold testing formula of a common soil, rock and other samples. In addition, bi 2O3 is used as a trapping agent, analysis procedures can be simplified through ash blowing, but platinum group elements in a plurality of black rocks are wrapped in Ni-Mo sulfide, part of metal elements such as Ni, cu and the like can enter bismuth buckles while Bi 2O3 traps noble metals, nickel skins can appear during one-time ash blowing, and the ash blowing process is seriously hindered. 10.0g of black rock sample is taken in the test, different gold test ingredients are added, and the conditions of slag formation, buckling and one-time ash blowing of the fire test gold are observed through melting at 1100 ℃, and the results are shown in Table 3. As can be seen from Table 3, the formula No. 5 can obtain a smooth and complete bismuth button with metallic luster, and the slag has the advantages of low melting point, small specific gravity, good fluidity, easy separation of the button slag, difficult breakage of the bismuth button and no nickel-plating effect of ash blowing.
TABLE 3 flux formulation for gold test
2. Selection of ash blowing mode
The general geological sample analysis Pt, pd, au, bismuth buckles formed after enrichment of bismuth test gold can obtain round noble metal silver beads through one-time ash blowing, but because the components of black rock are too complex, only non-granular loose silver flakes can be formed after one-time ash blowing and are adhered to a magnesia cupel, and cannot be taken out completely, so that the measurement result is low, as shown in figure 1. Through experiments, a certain amount of tellurium is added into a gold test batch, when the bismuth button is blown to about 5mm in a high-temperature furnace at 860 ℃ in a magnesia cupel, the magnesium is rapidly poured into a porcelain crucible or a porcelain crucible cover containing molten borax, secondary ash blowing is completed under the condition of borax wrapping, and round and bright tellurium-silver composite particles can be obtained after cooling, as shown in figure 2.
3. Bismuth oxide dosage test
10.0G of black rock standard substance GBW07737 parts are weighed, 20g, 30g, 40g and 50g of Bi 2O3 and a gold test ingredient are respectively added according to Table 4, and a dosage test of Bi 2O3 is carried out. And (3) determining Pt, pd and Au by dissolving and constant-volume ICP-AES after secondary ash blowing according to the experimental method flow of 1.3. As can be seen from the measurement results in Table 4, the Bi 2O3 is used in an amount of more than 30g under the conditions of reasonable alloy preparation and good slag fluidity, and the measurement results of Pt, pd and Au have no significant difference from the identification values, so that the addition amount of bismuth oxide is generally 40g in order to ensure the collection rate of noble metals.
TABLE 4 bismuth oxide dosage
4. Influence of the amount of Potassium nitrate on the formation of buttons and the enrichment of noble Metal elements
Because the black rock contains a large amount of carbon, sulfur, nickel and other elements, the gold is directly tested on the premise of not burning, and the complete bismuth button is difficult to form due to strong reducibility. And when bismuth button is ash blown once, a large amount of nickel skin appears, which seriously hinders the normal operation of ash blowing. Through the test, reducing the reducing agent flour in the formula, the carbon in the black rock is used as the reducing agent, and the buckling can not be realized, so the test selects to add the oxidizing agent potassium nitrate, and the buckling condition is adjusted. 8g, 10g, 12g and 15g of potassium nitrate are respectively added into the optimal gold test ingredients of 10g of black rock standard substance GBW07737 to be smelted at high temperature to form buckles, wherein when 8g and 10g of potassium nitrate bismuth buckles are added and subjected to primary ash blowing at 860 ℃, nickel skin is serious to be formed, the nickel skin is required to be pulled out in the ash blowing process to complete ash blowing, and the state after the ash blowing is shown in figure 3 as the consumption of potassium nitrate is increased and the primary ash blowing nickel skin is gradually reduced. From the ash blowing condition, when the dosage of potassium nitrate is 15g, the bismuth buckle is complete, and the nickel plating effect can be eliminated. By selecting the condition and carrying out a secondary ash blowing test, round and bright tellurium-silver composite particles can be obtained, the measurement results of Pt, pd and Au after the composite particles are subjected to acid dissolution are shown in table 5, and the measurement results show that when the adding amount of potassium nitrate is 15g, the measurement results are accurate and reliable.
TABLE 5 Potassium nitrate dosage test
5. Influence of iron powder on buckling and noble metal element enrichment
The black shale sample has higher sulfur content, the reducing force is not easy to master, the negligence of buckling is high, copper matte or yellow slag can be generated sometimes, the buckling is not aggregated, noble metal cannot be trapped quantitatively, the bismuth buckling property is fragile and fragile, the iron powder is added, the influence of sulfur can be effectively eliminated, the toughness of the bismuth buckling is increased, and the buckling is not fragile when the buckling slag is separated. 10g of black rock standard substance GBW07737 is weighed respectively, iron powder with different amounts is added into the optimal gold test ingredients according to the table 6, and the buckling condition and the influence of two times of ash blowing on the enrichment of noble gold elements are shown in the table 6. The result shows that the addition amount of the iron powder is more than 6g, the bright bismuth button which is not fragile can be obtained, the measurement results of Pt, pd and Au after secondary ash blowing are good, and 8g of iron powder is selected for test in order to ensure the recovery rate of Pt, pd and Au.
Table 6 iron powder dosage test
6. Effect of potassium tellurite on tellurium-silver composite particles
Ag. Te can be used as an ash blowing protective agent, but Te has strong oxidation resistance, a certain amount of Bi can be reserved in the grain combination during one ash blowing as long as Te exists, and the loss can be reduced due to the protection of Bi on noble metal elements. In addition, te can form a compound (such as PtTe 2) with noble metal and also plays a role in protection. Experiments show that the bismuth button with only silver nitrate can only form flat and rough silver flakes during secondary ash blowing, see fig. 4, and the ash blowing time is slightly long, so that the silver flakes disappear. The bismuth button obtained by adding 0.5mL of 60g/L AgNO 3 and 0.5mL of 76g/L K 2TeO3 through experiments can form smooth and round tellurium-silver aggregate particles through secondary ash blowing, and is shown in figure 5. The determination results of Pt, pd and Au after acid dissolution have no obvious difference from the identification values.
7. Detection limit and linear equation of method
Preparing a Pt, pd and Au mixed standard working solution by using 5% (V/V) aqua regia as a medium according to a table 7, measuring the corresponding spectral line intensity under the optimal instrument condition, and drawing a calibration curve, wherein a linear regression equation, a correlation coefficient and a linear range are shown in the table 7. The full-flow 12 independent blank tests were performed according to the experimental method, and the detection limit of the method was calculated with 3 times of standard deviation, and the results are shown in table 7.
TABLE 7 Linear Range, linear equation, correlation coefficient and detection limit
8. Recovery rate of the process
10.0G of black rock standard substance GBW07737 is weighed, different amounts of Pt, pd and Au standard solutions are respectively added, smelting and ash blowing are carried out according to an experimental method, and the standard adding recovery rate is calculated, and the result is shown in Table 8. Experiments show that the recovery rates of Pt, pd and Au are all more than 97%.
Table 8 method recovery test
9. Precision and accuracy of the method
Black rock standard substances GBW07736 and GBW07737 and copper nickel sulphide ore standard substances GBW07194 and GBW07195 with higher carbon and sulfur content are selected, the black rock standard substances GBW07736 and GBW07737 and the copper nickel sulphide ore standard substances GBW07194 and GBW07195 are analyzed for 12 times in parallel according to an experimental method, and the precision and the accuracy of the method are examined, and the results are shown in Table 9. The results show that the Relative Error (RE) between the standard substance measurement result and the identification value is-4.31% -3.77%, and the Relative Standard Deviation (RSD) is less than 6.92%.
Precision and accuracy of the method of table 9 (n=12)
While the invention has been described with reference to the embodiments, those skilled in the art will understand that various specific parameters in the above embodiments may be changed without departing from the spirit of the invention, and thus a plurality of specific embodiments are common variation ranges of the invention, and will not be described in detail herein.
Claims (1)
1. The platinum-palladium-gold gray blowing method in black rock with tellurium-silver as a protective agent is characterized by comprising the following steps of:
(1) Enrichment of bismuth gold test: adding a gold test ingredient into a 10.0 g black shale sample, wherein the gold test ingredient consists of borax, sodium carbonate, silicon dioxide, bismuth oxide, wheat flour, potassium nitrate, iron powder and a covering agent, 15g of borax, 50g of sodium carbonate, 10g of silicon dioxide, 40g of bismuth oxide, 2g of wheat flour, 15g of potassium nitrate, 8g of iron powder and 5g of covering agent are needed based on the 10.0 g black shale sample, and the covering agent is silicon carbide and light magnesium oxide; dropwise adding 0.5 mL of 60 g/L AgNO 3 solution and 0.5 mL of 76 g/L K 2TeO3 solution, fully mixing, pouring into a clay crucible, uniformly adding a layer of SiC and light MgO mixed covering agent, placing the clay crucible into a gold test furnace at 800 ℃, heating to 20 min, continuously raising the furnace temperature to 1100 ℃, melting for 30 min, taking out the crucible while the clay crucible is hot, pouring the molten mass into an iron mold, cooling, smashing a glass body, and taking out a bismuth button;
(2) Primary ash blowing: preheating a magnesia cupel in a high-temperature furnace at 900 ℃ for 1h, taking out, immediately placing a bismuth button in the cupel, putting the cupel in the high-temperature furnace again, adjusting the furnace temperature to 860 ℃, closing a furnace door for 1-2 min, opening the furnace door for 2-3 cm, leading air into a furnace chamber, and carrying out primary ash blowing;
(3) Secondary ash blowing: when the primary ash blowing is over, the porcelain crucible containing 2-3 g of borax is put into a high temperature furnace to be melted, when bismuth button ash is blown to the diameter of 5 mm, the bismuth button is rapidly poured into the porcelain crucible containing the melted borax, secondary ash blowing is continued, when the grain diameter is 1-2 mm, the crucible is taken out, naturally cooled, smashed and tellurium-silver grains are taken out.
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